Retention behaviour of quinolone derivatives in high-performance liquid chromatography

Barbosa, J.; Bergés, Rosa; Sanz‐Nebot, Victoria

doi:10.1016/s0021-9673(98)00428-2

Cited by 71 publications

(35 citation statements)

References 39 publications

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“…In previous work [18,38,45,46] Cls and polymeric columns have been used but in this work the best results were obtained by use of a Cs column. Although acetonitrile-water mixtures are suitable for chromatography of quinolones [9,18,45], good peak symmetry is obtained only if an organic competing base or an ammonium salt is added [9].…”

Section: Resultsmentioning

confidence: 91%

Optimization of the composition and pH of the mobile phase used for separation and determination of a series of quinolone antibacterials regulated by the European Union

et al. 2002

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SummaryTo ensure the safety of human food the European Union (EU) has set tolerance levels for quinolone compounds in animal products, so screening and confirmatory analytical methods are required for monitoring of these drugs. In this work, the proportion of organic modifier and the pH of acetonitrile-water mixtures used as mobile phases were optimized for separation of a group of quinolones. Linear solvation energy relationship (LSER) formalism based on the single solvent polarity parameter E N was used to predict the chromatographic behaviour of the compounds as a function of the amount of acetonitrile in the mobile phase. Correlation bef,,veen retention and the pH of aqueous-organic mobile phases has also been used to optimize mobile-phase pH. The optimized mobile phase was a hnear gradient starting from 18:82 (v/v) acetonitrileacetate + formate buffer, pH 2.5. Quality data were determined and were satisfactory The method detection hmitwas approximately 10 ng mL 1 for most of the quinolones studied. The proposed mobile phase is compatiblewith mass spectrometric detection of the substances.

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Section: Resultsmentioning

confidence: 91%

Optimization of the composition and pH of the mobile phase used for separation and determination of a series of quinolone antibacterials regulated by the European Union

et al. 2002

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“…The isoelectric point is therefore at pH = 7.70. In 50:50 v/v acetonitrile-water solvent Barbosa et al 14 reported the dissociation constants of fleroxacin pK 1 = 6.97 ± 0.02 and pK 2 = 8.21 ± 0.03 determined potentiometrically and pK 1 = 6.32 ± 0.05 and pK 2 = 8.05 ± 0.05 determined by HPLC. Our values are in fair agreement with the potentiometric ones.…”

Section: Resultsmentioning

confidence: 99%

Validation of an HPLC Method for the Determination of Fleroxacin and Its Photo‐degradation Products in Pharmaceutical Forms

2004

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HPLC determination of fleroxacin in dosage forms was carried out using either reversed-phase column YMC pack ODS-AQ or Supelco LC Hisep shielded hydrophobic phase column, with UV detection at 280 nm. The mobile phase for ODS column consisted of 50:50:0.5 v/v/v and for Hisep column 15:85:0.5 v/v/v acetonitrile-water-triethylamine. The pH of the mobile phase was adjusted to 6.30 for ODS column and to 6.85 for Hisep column, with H3PO4. Linear response was obtained in the concentration range of fleroxacin between 0.01 and 1.30 micrograms/mL. Detection limit was 4.8 ng/mL. Recovery test in the determination of fleroxacin in "Quinodis" tablets (Hoffmann La Roche, nominal mass 400 or 200 mg) was 98-101% for both columns. The effect of the composition and pH of the mobile phase on spectra, retention time and dissociation constants of fleroxacin was discussed. The proposed method could be also used for separation of the photo-degradation products of fleroxacin. Ten degradation products were separated on the ODS-AQ column, thus confirming the suitability of the proposed method for stability study of fleroxacin in pharmaceuticals.

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“…The pH of the mobile phase is a major factor influencing the chromatographic behaviour of FQs, given that they contain ionogenic functions such as carboxylic acid and amino groups [15]. The carboxyl group is normally a stronger acid than the ammonium group.…”

Section: Optimization Of Hplc Conditionsmentioning

confidence: 99%

“…Piperazinylquinolones have two pK a values, pK a1 L 6, and pK 2a L 9 for the carboxylic function and the piperazinyl moiety, respectively [18]. The mobile phase pH contributes for a highest fluorescence, since they exist mostly in cationic form at acidic pH.…”

Section: Optimization Of Hplc Conditionsmentioning

confidence: 99%

Determination of fluoroquinolone antibiotics in surface waters from Mondego River by high performance liquid chromatography using a monolithic column

Pena

Chmielova

Lino

et al. 2007

J of Separation Science

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Short CommunicationDetermination of fluoroquinolone antibiotics in surface waters from Mondego River by high performance liquid chromatography using a monolithic column A novel LC -fluorescence detection method based on the use of a monolithic column for the determination of norfloxacin, ciprofloxacin, and enrofloxacin antibiotic residues in environmental waters was developed. Fluoroquinolones (FQs) were isocratically eluted using a mobile phase consisting of 0.025 M phosphoric acid solution at pH 3.0 with tetrabutylammonium and methanol (960:40, v/v) through a Chromolith Performance RP-18e column (10064.6 mm) at a flow rate of 2.5 mL/min and detected at excitation and emission wavelengths of 278 and 450 nm, respectively. After acidification and addition of EDTA, water samples were extracted using an Oasis HLB cartridge. Linearity was evaluated in the range of 0.05 to 1 lg/mL and correlation coefficients of 0.9945 for norfloxacin, 0.9974 for ciprofloxacin, and 0.9982 for enrofloxacin were found. The limit of quantification was 25 ng/L for the three FQs. The recovery of FQs spiked into river water samples at 25, 50, and 100 ng/ L fortification levels ranged from 76.5 to 91.0% for norfloxacin, 78.5 to 97.2% for ciprofloxacin, and 79.4 to 93.6% for enrofloxacin. This method was successfully applied to the analysis of water samples from the Mondego River, and ciprofloxacin and enrofloxacin residues were detected in eight water samples.

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Retention behaviour of quinolone derivatives in high-performance liquid chromatography

Cited by 71 publications

References 39 publications

Optimization of the composition and pH of the mobile phase used for separation and determination of a series of quinolone antibacterials regulated by the European Union

Optimization of the composition and pH of the mobile phase used for separation and determination of a series of quinolone antibacterials regulated by the European Union

Validation of an HPLC Method for the Determination of Fleroxacin and Its Photo‐degradation Products in Pharmaceutical Forms

Determination of fluoroquinolone antibiotics in surface waters from Mondego River by high performance liquid chromatography using a monolithic column

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